1、 FORD LABORATORY TEST METHOD AK 118-01 Date Action Revisions 2001 01 22 Revised Editorial no technical change A. Cockman 2000 03 30 Revised Editorial no technical change A. Cockman 1994 01 03 Printed copies are uncontrolled Page 1 of 8 Copyright 2001, Ford Global Technologies, Inc. GENERAL PROCEDURE
2、S FOR EVALUATION OF A CLEANER Application This procedure covers preparation of cleaners for analysis and a general qualitative evaluation of a cleaner. Apparatus Required Burner Bunsen, Fisher, Meker or equivalent. Erlenmeyer Flask Pipet 10 mL Volumetric Flask 1000 mL; calibrated Platinum Wire Beake
3、r 150 mL Watch Glass Used to cover 250 mL beaker Cobalt Glass The above apparatus is available from any reputable laboratory equipment supply house. Materials Required Nitric Acid Concentrated, Reagent grade; CAUTION: Corrosive* Hydrochloric Acid Concentrated, Reagent grade; CAUTION: Corrosive* FORD
4、 LABORATORY TEST METHOD AK 118-01 Page 2 of 8 Copyright 2001, Ford Global Technologies, Inc. Sulfuric Acid Concentrated, Reagent grade; CAUTION: Corrosive* Sodium Hydroxide Reagent grade; CAUTION: Corrosive* Ammonium Hydroxide Concentrated, Reagent grade; CAUTION: Corrosive* Barium Chloride Reagent
5、grade; CAUTION: Poisonous* Lead Acetate Reagent grade; CAUTION: Toxic* Methyl Alcohol Reagent grade; CAUTION: Low flash point* Diphenylamine Reagent grade; CAUTION: Flammable* Molybdic Acid 85 % concentration, Reagent grade Distilled Water CO2 -free; 20 micromhos/cm at 25 C max conductivity (ASTM D
6、1125) Turmeric Paper Red Litmus Paper * Refer to Industrial Hygiene for health and safety comments regarding the above materials. Solutions Required* Ammonium Carbonate or Ammonium Chloride Solution Ammonium carbonate (approx. 22 % solution): Dissolve 250 g of the powdered salt in 1.00 L of distille
7、d water containing 100 mL of concentrated NH4OH. Ammonium chloride (10 % solution): Dissolve 100 g of NH4CL in 1.00 L of distilled water. Barium Hydroxide Solution 5 % solution, dissolve 50 g of Ba(OH)2 8H2O in 1.00 L of distilled water. Ammonium Molybdate Solution Refer to FLTM AZ 102-01 FORD LABOR
8、ATORY TEST METHOD AK 118-01 Page 3 of 8 Copyright 2001, Ford Global Technologies, Inc. Ferrous Sulfate Solution Refer to FLTM AZ 102-01 Sodium Hydroxide Solution 1.0 Normal Silver Nitrate Solution 0.1 Normal Albumin Solution 1 % solution; dissolve 1 g of albumin in 100 mL of distilled water. Barium
9、Chloride Solution Dissolve 100 g of barium chloride in distilled water and dilute to 1.00 L. * Refer to Industrial Hygiene for health and safety comments. Conditioning and Test Conditions All test values indicated herein are based on material conditioned in a controlled atmosphere of 23 +/- 2 C and
10、50 +/- 5 % relative humidity for not less than 24 h prior to testing and tested under the same conditions unless otherwise specified. Procedure 1. Preparation of Samples for Analysis A. Solids The selection of a representative sample is a necessary prerequisite for any accurate analysis. This is par
11、ticularly important with the alkalies since they are susceptible to rapid contamination by moisture and carbon dioxide upon exposure to air. They are also usually not uniform in particle size and tend to segregate on handling. Samples in flake or powdered form must be thoroughly mixed and quartered.
12、 All operations must be carried out rapidly with a minimum exposure to air. In the case of heterogeneous materials containing large particles, it is advisable to screen a large sample, grind the coarse fraction, and recombine the two fractions, followed by thorough mixing and quartering. Place appro
13、ximately 50 g of the prepared sample into a weighing bottle, weigh the bottle and contents. Remove about 35 to 40 g to a 400 mL beaker. Dissolve rapidly in distilled water and rinse quantitatively into a calibrated 1000 mL volumetric flask. Close the flask at once, cool, make up to the mark at 23 +/
14、- 2 C with distilled water, and mix thoroughly. Reweigh the weighing bottle and remaining contents and take the weight of sample by difference. FORD LABORATORY TEST METHOD AK 118-01 Page 4 of 8 Copyright 2001, Ford Global Technologies, Inc. To prepare the sample for testing, an aliquot of this solut
15、ion is used to make the required 1 % solution for the analysis. B. LIQUIDS Pipet 10 mL of the concentrate into a calibrated 1000 mL volumetric flask. Dilute with distilled water at room temperature to the 1000 mL mark and mix thoroughly. This preparation is a 1 % solution by volume. The specific gra
16、vity of the concentrate is determined at 23 +/- 2 C in order to calculate the weight of sample used for determinations and reporting as percentages. Remarks: 1. When carbon dioxide determinations of highest accuracy are to be obtained, CO2-free distilled water must be used for dilutions. 2. When pH
17、values at approximately 6 - 7 are to be determined, neutral distilled water must be used. 3. Proper aliquots from the above dilutions are specified in the specification requirements. The “weight of sample“ in each determination refers to actual weight in grams of the substance in the aliquot. II Qua
18、litative Examination If the cleaner is an unknown as to a formulation, a qualitative examination for the constituents is made in order to determine what quantitative analysis must be made. It is not necessary to run an item if it is found to be absent. Normally, cleaners are either sodium salts or p
19、otassium salts and rarely a blend of the two. A flame test is used to determine if one or both of these alkalies are present. Acidify the alkaline solution with hydrochloric acid. Make a flame test with a platinum wire. An intense yellow flame indicates sodium. A pale violet flame indicates potassiu
20、m. If the flame is intense yellow, view it through cobalt glass. A red flame as thus viewed indicates potassium. To test for ammonium, take the sample in a small beaker, add sodium hydroxide solution in excess, cover the beaker with a watch glass containing on the underside a moist piece of red litm
21、us paper. Warm and observe the litmus paper. If it changes from red to blue, ammonium is present. Usually an Erlenmeyer flask with a bent tube is much safer to use since contact with the sodium hydroxide is eliminated. Chlorides Acidify with nitric acid and add silver nitrate. If a precipitate forms
22、, chlorides are present. Sulfates Acidify with nitric acid and add barium chloride. If a precipitate forms, sulfates are present. FORD LABORATORY TEST METHOD AK 118-01 Page 5 of 8 Copyright 2001, Ford Global Technologies, Inc. Borates 1. Treat the cleaner with methyl alcohol and then concentrated su
23、lfuric acid. Stir the mixture and ignite the alcohol; a green-bordered flame will appear if borates are present. 2. Acidify with hydrochloric acid and dip a strip of turmeric paper into this solution. Dry the paper a reddish-brown color shows the presence of borates. Moisten this strip with caustic
24、soda or ammonium hydroxide, the paper will turn bluish-colored. Phosphates Acidify with nitric acid, boil for a few minutes, cool to 23 +/- 2 C and add an excess of ammonium molybdate solution. Let stand. A yellow precipitate indicates the presence of phosphates. Addendum 1a Silver nitrate produces
25、a yellow precipitate of silver phosphate readily soluble in nitric acid and in ammonia. The precipitate, therefore, can be formed only in neutral solution. Ortho phosphates are indicated. 1b Silver nitrate gives a white, curdy precipitate, soluble in ammonia and nitric acid. Pyrophosphates are indic
26、ated. 1c Silver nitrate precipitates white silver metaphosphate, soluble in ammonia and nitric acid. 2. Albumin solution is coagulated by an aqueous solution of the free acid (difference from pyro and orthophosphoric acids), but not by a solution of alkali metaphosphate, except on the addition of ac
27、etic acid. Nitrites/ Diphenylamine in concentrated sulfuric acid will color the Nitrates material intensely blue if nitrites or nitrates are present. Other oxidizing agents will give the same reaction. Nitrites Place the material in a test tube with 5 mL of distilled water, add an equal volume of co
28、ncentrated acetic acid and cool to 23 +/- 2 C by shaking the solution under running water. Add about 5 mL of saturated ferrous sulfate solution. When a nitrite is present, a dark brown color will develop in the solution. The test is not reliable in the presence of an iodide or a chromate. Chromates
29、Lead acetate produces in solutions of normal chromates and dichromates a yellow precipitate which is soluble in nitric acid but insoluble in acetic acid. FORD LABORATORY TEST METHOD AK 118-01 Page 6 of 8 Copyright 2001, Ford Global Technologies, Inc. Silicates Usually detected at the same time as ph
30、osphates as evidenced by a yellow color in solution which can be seen when filtering out the phosphate. The silicate forms a complex salt with the ammonium molybdate. Precipitation using an ammonium salt - usually a solution of ammonium chloride or ammonium carbonate is mixed with the sample. The si
31、licates will be precipitated as the hydroxide. Carbonates Acidify with hydrochloric acid and watch closely to see if there is any sign of effervescence. If there is, observe if the escaping gas has any color. The presence of carbonates can be confirmed by using barium hydroxide solution. If a carbon
32、ate is present, the barium hydroxide will become turbid. III Physical Characteristics, pH, Surface Tension A. Physical Characteristics 1. Solid a. Powder, granule, crystal or lump b. Color c. Odor 2. Liquid a. Clear, opaque, emulsion or paste b. Color c. Odor B. pH Refer to ASTM E 70 C. Surface Tens
33、ion - Refer to ASTM D 1331 IV. A. Probable Formulation Calculations Phosphates: P2O5 X 2.3101 = Trisodium Phosphate Na3PO4 X 2.0003 = Disodium Phosphate Na2HPO4 X 1.8734 = Tetrasodium Pyrophosphate Na4P2O7 X 1.7278 = Sodium Tripolyphosphate Na5P3O10 X 1.4367 = Sodium Hexametaphosphate (NaPO3)6 X 1.4
34、367 = Sodium Trimetaphosphate (NaPO3)3 FORD LABORATORY TEST METHOD AK 118-01 Page 7 of 8 Copyright 2001, Ford Global Technologies, Inc. Carbonates: CO2 X 2.4083 = Sodium Carbonate Na2CO3 X 2.1588 = Sodium Sesquicarbonate Na3H(CO3)2 X 1.9089 = Sodium Bicarbonate NaHCO3 Silicates: SiO2 X 2.0316 = Sodi
35、um Metasilicate Na2SiO3 X 3.0632 = Sodium Orthosilicate Na4SiO4 Borates: B2O3 X 1.4451 = Sodium Tetraborate Na2B4O7 X 2.7389 = Borax Na2B4O7 10H2O X 1.7763 = Boric Acid H3BO3 Nitrites: NO2 X 1.4996 = Sodium Nitrite NaNO2 Nitrates: NO3 X 1.3708 = Sodium Nitrate NaNO3 Sulfates: SO4 X 1.4786 = Sodium S
36、ulfate Na2SO4 Chlorides: Cl X 1.6485 = Sodium Chloride NaCl B. Titratable Alkalinity as Na2O Various salts contribute to the alkalinity of a cleaner. Some are tabulated below: Sodium Carbonate (Na2CO3) 0.5849 Sodium Hydroxide (NaOH) 0.7748 Sodium Metasilicate (Na2SiO3) 0.5079 Trisodium Phosphate (Na
37、3PO4) 0.3781 Disodium Phosphate (Na2HPO4) 0.2183 Tetrasodium Pyrophosphate (Na4P2O7) 0.2331 Sodium Tripolyphosphate (Na5P3O10) 0.1685 Sodium Hexametaphosphate (NaPO3)6 None Sodium Trimetaphosphate (NaPO3)3 None Sodium Tetraborate (Na2B4O7) 0.3088 Sodium Orthosilicate (Na4SiO4) 0.6735 FORD LABORATORY
38、 TEST METHOD AK 118-01 Page 8 of 8 Copyright 2001, Ford Global Technologies, Inc. FLTMs that are Useful for Cleaner Analysis: AK 101-01 Determination of Buffer Value of Soap AK 103-01 Determination of Percent Nitrite in Cleaners AK 103-02 Quantitative Analysis of Nitrite (as NO2) in Cleaners AK 105-
39、01 Determination of Volatile and Non-volatile Matter in Cleaners AK 106-01 Quantitative Analysis of the Total Alkalinity of Cleaners AK 107-01 Quantitative Analysis of Caustic Soda or Caustic Potash in Cleaners AK 108-01 Quantitative Analysis of Combined & Free Ammonia in Ammonium Salts in Cleaners
40、AK 109-01 Quantitative Analysis of Phosphates in Cleaners AK 110-01 Quantitative Analysis of Carbonates (As CO2) in Cleaners AK 111-01 Quantitative Analysis of Borates in Cleaners AK 112-01 Quantitative Analysis of Silicates in Cleaners AK 113-01 Quantitative Analysis of Nitrate (As NO3) in Cleaners
41、 AK 114-01 Quantitative Analysis of Sulfates in Cleaners AK 115-01 Quantitative Analysis of Chlorides in Cleaners AK 116-01 Quantitative Analysis of Surfactants and Wetting Agents in Cleaners AK 117-01 Quantitative Analysis of Solvent Content of Cleaners Chemicals, materials, parts, and equipment referenced in this document must be used and handled properly. Each party is responsible for determining proper use and handling in its facilities.
